CN100355699C - Process for making graphite powder with electromagnetic property - Google Patents
Process for making graphite powder with electromagnetic property Download PDFInfo
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- CN100355699C CN100355699C CNB2006100396610A CN200610039661A CN100355699C CN 100355699 C CN100355699 C CN 100355699C CN B2006100396610 A CNB2006100396610 A CN B2006100396610A CN 200610039661 A CN200610039661 A CN 200610039661A CN 100355699 C CN100355699 C CN 100355699C
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Abstract
The present invention discloses a preparation method of graphite powder with electromagnetic properties. In the method, a graphite solution and a Fe<2+>/Fe<3+> mixed solution are uniformly mixed, then the obtained mixed solution is poured into a three-mouth flask arranged in a thermostatic waterbath, alkali liquid is added in the mixed solution for reaction till the solution is alkaline, after the reaction, the solution is moved to another higher thermostatic waterbath for crystallization for a period of time, and after washing and sample drying, the graphite powder attached with magnetic nanoparticles is obtained. The method has the advantages of simple preparation process, low production cost and suitability for industrial production; the prepared magnetic graphite powder has the advantages of favorable electroconductibility and magnetoconductivity, and is a superior raw material of electromagnetic shielding materials; the powder has favorable application prospects in the fields of electronics, electricity, communication, aviation, military affairs, etc.
Description
Technical field
The invention belongs to the powder preparing technical field, a kind of graphite powder Preparation Method that is used for electromagnetic shielding, has conductive magneto-conductive of more specifically saying so.
Background technology
Along with electronic industry and science and technology development, the generally use of various electronic electric equipments and electronic product, electromagnetic wave outside radiating electromagnetic energy increases gradually with the speed of annual 7%-14%, electromagnetic environment is polluted serious day by day, on the other hand, electronic product and electronic electric equipment are to digitizing, Highgrade integration, signal level small quantization direction develops, they are the susceptibility increase of electromagnetic environment to external world, be subjected to outside electromagnetic interference easily and produce flase operation, image distortion, disturb radio communication etc., brought for people's production and life and seriously influence.Electromagnetic shielding is the important means of anti-electromagnetic interference, traditional electromagnetic shielding material mainly is top layer conductivity type shielding material and fills compound shielding material, and top layer conductive shield material is conductive filler materials such as metal-powder, carbon black and macromolecular material to be mixed with form or make acquisition very thin conductive metal layer in insulating material surface reach the effect of shielding by physico-chemical process.Fill composite shielding material and be the electromagnetic shielding material that processes through injection or extrusion moulding by macromolecule matrix and conductive filler material.Though these traditional shielding materials can reach the effect of shielding, shielding properties is general, and the frequency band range of shielding is very narrow, thereby has limited the application of these shielding materials.According to the electromagnetic shielding theory, the electromagnetic shielding material of excellent property should have higher electric conductivity and permeability.And novel shielding material is when emphasizing to shield bandwidth and high shielding properties, and the shielding material that development quality is light is the emphasis of present this area research.
Graphite is that a kind of good conductive filler material, particularly graphite prepared expanded graphite behind intercalation has high specific conductivity and big surface-area, thereby has given expanded graphite good capability of electromagnetic shielding.D.D.L.Chung suppresses expanded graphite by high pressure graphite gasket has advantages of favorable electromagnetic shielding effect, and this material also has good thermostability, chemical stability and low thermal expansivity, but the shielding material of Zhi Zaoing is diamagnetic thus, thereby the shielding frequency range of this material is very limited.In order to improve the graphite-based shielding material in the deficiency aspect this, a lot of research workers consider to add magnetic substance to improve the shielding properties of graphite-based shielding material in graphite.Peng Junfang etc. are with expanded graphite and Fe (OH)
3Mix, at high temperature expanded fast then, made the graphite-base composite material of the ferriferous oxide that contains ferrimagnetism, this material has electroconductibility and ferrimagnetism, its shielding properties increases, especially the pure relatively graphite of the shielding frequency range of this material has had large increase, but because magnetic particle is that ferrimagnetism and diameter of particle are bigger, is difficult to reach the ideal shield effectiveness.
Summary of the invention
Purpose of the present invention provides a kind of preparation method with powdered graphite of electromagnetic property, and the graphite-based shielding material made from the powdered graphite that utilizes the inventive method to make has shielding properties and comparatively ideal shielding frequency range preferably.
Technical scheme of the present invention is such: a kind of preparation method with powdered graphite of electromagnetic property, realize as follows:
One, take by weighing a certain amount of graphite and be scattered in the liquid medium, form the graphite dispersion liquid, wherein, the weight ratio of graphite and liquid medium is 1: 10-1000;
Two, in molar ratio 2.0: 1-5.5: 1 takes by weighing divalent iron salt, trivalent iron salt, and being mixed with concentration is the iron ion mixing solutions of 0.2-0.8M;
Three, be 1 with above-mentioned graphite dispersion liquid and iron ion mixing solutions with volume ratio: 1-6: after 1 the mixed, be placed in 29 ℃ of-31 ℃ of waters bath with thermostatic control, and stir 10-20min, it is mixed;
Four, adding concentration in the mixing solutions of step 3 gained is the alkali lye of 0.3-0.6M, and the stirring that does not stop is alkalescence until solution;
Five, the solution of step 4 gained is moved in 35 ℃ of-50 ℃ of waters bath with thermostatic control crystallization 1-3 hour;
Six, the solution after the washing crystallization is neutral until washings, adopts magnetic separation technique to isolate throw out in the solution at last, and oven dry, pulverizing have promptly obtained being attached with magnetic Fe
3O
4The powdered graphite of nanoparticle.
Liquid medium in the above-mentioned steps one is the organic or inorganic solution that easily dissolves graphite.
In the above-mentioned steps two, divalent iron salt and trivalent iron salt are the molysite that does not contain the strong oxidizing property acid group.
Above-mentioned divalent iron salt is FeCl
2Or FeSO
4
Above-mentioned trivalent iron salt is FeCl
3Or Fe
2(SO4)
3
In the above-mentioned steps four, the alkali lye that adds in mixing solutions is middle aqueous alkali.
After adopting such scheme, the powdered graphite of the present invention's preparation has the characteristic of conduction, magnetic conduction concurrently, has remedied that conventional graphite only has electroconductibility and the deficiency that do not have magnetic; And preparation technology of the present invention simple, be easy to industrialization production.Prepare electromagnetic shielding material with the powdered graphite of the present invention preparation and have characteristics such as low, in light weight, the super wide frequency range inner shield of density is effective, can be applicable to the broadband electromagnetical shielding material in electromagnetic interference, electromagnetic pollution, communication and the areas of information technology, good application prospects is arranged in electronics, electric, communication, aviation and military field.
Description of drawings
The Fe that Fig. 1 prepares for the inventive method
3O
4The sem photograph of/NG nano-complex particle.
The Fe that Fig. 2 prepares for the inventive method
3O
4The energy spectrogram of/NG nano-complex particle.
The Fe that Fig. 3 prepares for the inventive method
3O
4The hysteresis curve of/NG nano-complex particle.
Embodiment
A kind of preparation method with powdered graphite of electromagnetic property of the present invention, can realize by following several embodiment:
Embodiment 1:
1) takes by weighing the graphite alcohol dispersion liquid that 0.5000g2000 order graphite is mixed with 50ml; Take by weighing 0.8341gFeSO
4.6H
2O, 0.1622gFeCl
3.7H
2O is mixed with the mixing solutions of 50ml molysite.
2) pour into above-mentioned two kinds of solution in the open there-necked flask, place 30 ℃ of water-baths, and stirred 15 minutes, it is mixed with agitator.
3) to step 2) the mixed solution and dripping concentration of gained is the NaOH solution of 0.4mol/l, stirred solution ceaselessly when dripping NaOH solution is until the PH=12 of solution.
4) solution of step 3) gained was transferred in 50 ℃ of water-baths crystallization 2 hours, then with distilled water wash repeatedly with the throw out that obtains after the crystallization, until the PH=7 of washings.
5) adopt magnetic separation technique that throw out is separated, isolated throw out is dried, pulverize and just obtained being attached with Fe with vacuum drying oven
3O
42000 order powdered graphites of magnetic nano-particle.
Embodiment 2:
1) takes by weighing the graphite alcohol dispersion liquid that 0.5000g7000 order graphite is mixed with 50ml, take by weighing 0.8341gFeSO
4.6H
2O, 0.1622gFeCl
3.7H
2O is mixed with the mixing solutions of 50ml molysite.
2) pour into above-mentioned two kinds of solution in the open there-necked flask, place 30 ℃ of water-baths, and stirred 15 minutes, it is mixed with agitator.
3) to step 2) the mixed solution and dripping concentration of gained is the NaOH solution of 0.5mol/l, stirred solution ceaselessly when dripping NaOH solution is until the PH=13 of solution.
4) solution of step 3) gained was transferred in 35 ℃ of water-baths crystallization 2 hours, then with distilled water wash repeatedly with the throw out that obtains after the crystallization, until the PH=7 of washings.
5) adopt magnetic separation technique that throw out is separated, isolated throw out is dried, pulverize and just obtained being attached with Fe with vacuum drying oven
3O
47000 order powdered graphites of magnetic nano-particle.
Embodiment 3:
1) takes by weighing the graphite alcohol dispersion liquid that the 0.5000g nano-graphite is mixed with 50ml, take by weighing 0.8341gFeSO
4.6H
2O, 0.1622gFeCl
3.7H
2O is mixed with the mixing solutions of 50ml molysite.
2) pour into above-mentioned two kinds of solution in the open there-necked flask, place 30 ℃ of water-baths, and stirred 1 minute, it is mixed with agitator.
3) to step 2) the mixed solution and dripping concentration of gained is the NaOH solution of 0.4mol/l, stirred solution ceaselessly when dripping NaOH solution is until the PH=12 of solution.
4) solution of step 3) gained was transferred in 50 ℃ of water-baths crystallization 2 hours, then with distilled water wash repeatedly with the throw out that obtains after the crystallization, until the PH=7 of washings.
5) adopt magnetic separation technique that throw out is separated, isolated throw out is dried, pulverize and just obtained being attached with Fe with vacuum drying oven
3O
4The nano-graphite powder of magnetic nano-particle.
Embodiment 4:
1) takes by weighing the graphite alcohol dispersion liquid that the 0.5000g nano-graphite is mixed with 50ml, take by weighing 0.8341gFeSO
4.6H
2O, 0.1622gFeCl
3.7H
2O is mixed with the mixing solutions of 50ml molysite.
2) pour into above-mentioned two kinds of solution in the open there-necked flask, place 30 ℃ of water-baths, and stirred 15 minutes, it is mixed with agitator.
3) to step 2) the mixed solution and dripping concentration of gained is the NH of 0.5mol/l
3.H
2O solution is dripping NH
3.H
2Stirred solution ceaselessly in the time of O solution is until the PH=12 of solution.
4) solution of step 3) gained was transferred in 50 ℃ of water-baths crystallization 1 hour, then with distilled water wash repeatedly with the throw out that obtains after the crystallization, until the PH=7 of washings.
5) adopt magnetic separation technique that throw out is separated, isolated throw out is dried, pulverize and just obtained being attached with Fe with vacuum drying oven
3O
4The nano-graphite powder of magnetic nano-particle.
A kind of preparation method with powdered graphite of electromagnetic property of the present invention, can realize by following several embodiment: it is prepared is attached with Fe
3O
4The characteristic of the powdered graphite of magnetic nano-particle has the characteristic of conduction, magnetic conduction concurrently as shown in Figure 1, 2, 3, prepares electromagnetic shielding material with it and has characteristics such as low, in light weight, the super wide frequency range inner shield of density is effective.
Claims (6)
1, a kind of preparation method with powdered graphite of electromagnetic property is characterized in that: realize as follows:
One, take by weighing a certain amount of graphite and be scattered in the liquid medium, form the graphite dispersion liquid, wherein, the weight ratio of graphite and liquid medium is 1: 10-1000;
Two, in molar ratio 2.0: 1-5.5: 1 takes by weighing divalent iron salt, trivalent iron salt, and being mixed with concentration is the iron ion mixing solutions of 0.2-0.8M;
Three, be 1 with above-mentioned graphite dispersion liquid and iron ion mixing solutions with volume ratio: 1-6: after 1 the mixed, be placed in 29 ℃ of-31 ℃ of waters bath with thermostatic control, and stir 10-20min, it is mixed;
Four, adding concentration in the mixing solutions of step 3 gained is the alkali lye of 0.3-0.6M, and the stirring that does not stop is alkalescence until solution;
Five, the solution of step 4 gained is moved in 35 ℃ of-50 ℃ of waters bath with thermostatic control crystallization 1-3 hour;
Six, the solution after the washing crystallization is neutral until washings, adopts magnetic separation technique to isolate throw out in the solution at last, and oven dry, pulverizing have promptly obtained being attached with magnetic Fe
3O
4The powdered graphite of nanoparticle.
2, a kind of preparation method with powdered graphite of electromagnetic property according to claim 1 is characterized in that: the liquid medium in the above-mentioned steps one is the organic or inorganic solution that easily dissolves graphite.
3, a kind of preparation method with powdered graphite of electromagnetic property according to claim 1 is characterized in that: in the above-mentioned steps two, divalent iron salt and trivalent iron salt are the molysite that does not contain the strong oxidizing property acid group.
4, a kind of preparation method with powdered graphite of electromagnetic property according to claim 3, it is characterized in that: above-mentioned divalent iron salt is FeCl
2Or FeSO
4
5, a kind of preparation method with powdered graphite of electromagnetic property according to claim 3, it is characterized in that: above-mentioned trivalent iron salt is FeCl
3Or Fe
2(SO4)
3
6, a kind of preparation method with powdered graphite of electromagnetic property according to claim 1 is characterized in that: in the above-mentioned steps four, the alkali lye that adds in mixing solutions is middle aqueous alkali.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100396610A CN100355699C (en) | 2006-04-07 | 2006-04-07 | Process for making graphite powder with electromagnetic property |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100396610A CN100355699C (en) | 2006-04-07 | 2006-04-07 | Process for making graphite powder with electromagnetic property |
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| Publication Number | Publication Date |
|---|---|
| CN1837148A CN1837148A (en) | 2006-09-27 |
| CN100355699C true CN100355699C (en) | 2007-12-19 |
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|---|---|---|---|
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5452847B2 (en) * | 2007-03-22 | 2014-03-26 | スリーエム イノベイティブ プロパティズ カンパニー | Electromagnetic shielding material and sheet |
| CN102553521B (en) * | 2010-12-29 | 2015-09-09 | 合肥杰事杰新材料股份有限公司 | A kind of preparation method of magnetic graphite |
| CN102352215A (en) * | 2011-07-28 | 2012-02-15 | 西北工业大学 | Preparation method of electromagnetic double-complex nanometer microwave absorbent Fe3O4/NanoG |
| US20140225039A1 (en) * | 2013-02-11 | 2014-08-14 | Industrial Technology Research Institute | Radiation shielding composite material including radiation absorbing material and method for preparing the same |
| CN106583737A (en) * | 2016-11-17 | 2017-04-26 | 安徽荣玖智能装备科技有限公司 | Dense powder metallurgy magnetic ring not prone to cracking and suitable for magnetic water pump of new energy automobile and manufacturing method thereof |
| CN114525028B (en) * | 2021-09-26 | 2023-02-21 | 北京理工大学 | Adjustable polymer-based porous electromagnetic shielding material, and preparation method and application thereof |
| CN114390883B (en) * | 2022-01-10 | 2023-03-14 | 北京理工大学 | Throwing distributed electromagnetic damage cloud cluster and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1212473A (en) * | 1997-09-25 | 1999-03-31 | 中国科学院长春应用化学研究所 | Preparation of lithium ion battery carbon material negative pole |
-
2006
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1212473A (en) * | 1997-09-25 | 1999-03-31 | 中国科学院长春应用化学研究所 | Preparation of lithium ion battery carbon material negative pole |
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